石化厂溢油源快速查找的气相色谱指纹方法研究
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摘要
换热器物料泄漏一直是困扰石化企业的一个技术难题，传统的查漏方法费时费力。针对这种情况，本论文根据环境溢油源的查找原理，基于色谱技术建立了一个快速的查找泄漏源的方法，首次将固相微萃取这种新型的样品预处理技术和指纹的自动识别技术应用于此方法中。
固相微萃取(SPME)集采样、萃取、浓缩、进样于一体，快速、简便、无须有机溶剂，尤其它较高的灵敏度能使人们能够更早地发现泄漏源。本论文详细地研究了SPME的实验条件，讨论了萃取时间，萃取温度，解吸时间，解吸温度等因素对SPME的影响。使SPME在优化的条件下最大地发挥它的优越性。
在建立好的实验条件下，本论文对某石化厂各个换热器中的物料进行了研究，得到了每个换热器物料的色谱指纹，提出了特征指纹提取的5个原则，对其特征进行了研究。这些特征不仅能够充分反映各个换热器的物料区别，而且在封闭的系统中具有很好的稳定性。然后又首次将指纹的自动识别技术应用于换热器的查漏中，实现了特征指纹的计算机自动识别，可以节省大量的人力、物力。
最后，应用本论文建立的查漏方法，对一次实际泄漏事故进行研究，快速地查找到了泄漏源，证明此方法鉴别能力强，准确性好，分析迅速，操作简单，适合我国的国情，在换热器泄漏源的查找中具有很好的应用前景。
The leakage of the substances in the heat exchanger has been always bothering the petrochemical plant. The traditional method designed to detect the source of substances leakage is time consuming and laborious, In order to solve this problem,
in this paper a rapid method has been developed based on the gas chromatographic
technique. Solid phase microextraction (SPME) and auto identification of figure-print were firstly used in the leakage source detecting.
SPME is a kind of new method used in the pretreatment of the samples. It integrates sampling , extraction, concentration, and sample introduction into a single step. It has a number of advantages: fast, simple, sensitive, solvent-free etc, which can makes us find the leakage earlier than before. In this study, the conditions of SPME was optimized, including extraction time, extraction temperature, desorption time and desorption temperature, etc.
By using the method established, the chromatographic finger-prints of the substances in the heat exchanger in one petrochemical plant have been investigated in details . The character of the finger-print for each exchanger was extracted based on the chromatograms. Then auto identification method of spill-oil sources was developed here, less time and less labor are required than before.
Finally, a practical leakage event was investigated, the result shows that the method established in this paper is fast, simple, accurate and suitable to our country. It is very promising in the leakage detecting of the petrochemical plant.
固相微萃取(SPME)集采样、萃取、浓缩、进样于一体，快速、简便、无须有机溶剂，尤其它较高的灵敏度能使人们能够更早地发现泄漏源。本论文详细地研究了SPME的实验条件，讨论了萃取时间，萃取温度，解吸时间，解吸温度等因素对SPME的影响。使SPME在优化的条件下最大地发挥它的优越性。
在建立好的实验条件下，本论文对某石化厂各个换热器中的物料进行了研究，得到了每个换热器物料的色谱指纹，提出了特征指纹提取的5个原则，对其特征进行了研究。这些特征不仅能够充分反映各个换热器的物料区别，而且在封闭的系统中具有很好的稳定性。然后又首次将指纹的自动识别技术应用于换热器的查漏中，实现了特征指纹的计算机自动识别，可以节省大量的人力、物力。
最后，应用本论文建立的查漏方法，对一次实际泄漏事故进行研究，快速地查找到了泄漏源，证明此方法鉴别能力强，准确性好，分析迅速，操作简单，适合我国的国情，在换热器泄漏源的查找中具有很好的应用前景。
The leakage of the substances in the heat exchanger has been always bothering the petrochemical plant. The traditional method designed to detect the source of substances leakage is time consuming and laborious, In order to solve this problem,
in this paper a rapid method has been developed based on the gas chromatographic
technique. Solid phase microextraction (SPME) and auto identification of figure-print were firstly used in the leakage source detecting.
SPME is a kind of new method used in the pretreatment of the samples. It integrates sampling , extraction, concentration, and sample introduction into a single step. It has a number of advantages: fast, simple, sensitive, solvent-free etc, which can makes us find the leakage earlier than before. In this study, the conditions of SPME was optimized, including extraction time, extraction temperature, desorption time and desorption temperature, etc.
By using the method established, the chromatographic finger-prints of the substances in the heat exchanger in one petrochemical plant have been investigated in details . The character of the finger-print for each exchanger was extracted based on the chromatograms. Then auto identification method of spill-oil sources was developed here, less time and less labor are required than before.
Finally, a practical leakage event was investigated, the result shows that the method established in this paper is fast, simple, accurate and suitable to our country. It is very promising in the leakage detecting of the petrochemical plant.
引文
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[56] 范仪毅，冯钰琦，达世禄，色谱 2001，19(6)，497
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